气相色谱-嗅闻-质谱联用分析烟熏液中的挥发性风味物质

通过气相色谱-质谱-嗅闻(GC-O-MS)联用技术对国外优质烟熏液的风味物质进行分析,共检测出114种化合物,其中具有烟熏风味的酚类化合物23种,对烟熏液上色效果有重要影响的羰基化合物50种,此外还检测到酯类10种、醇类5种、烃类7种、杂环化合物14种,未知化合物5种.     

山楂核烟熏液(SF1)风味成分的分离剖析

山楂核烟熏液(SF1)为我国首次研制出的食用烟熏香味料。本文将SF1粗分成1～5号组分,然后运用GC/MS(气相色谱质谱联用法)进行分离分析。并通过谱图解析,计算机检索,标样核对及文献对照等方法鉴定出了73种化合物。其中酚类17种,酸类17种,羰基化合物14种,呋喃类8种,醇类8种,醚类4种,其他化合物5种。并进行了简单的感官试验。     

固相萃取辅助提取-气相色谱-质谱分析烟熏腊猪肉香气成分

采用固相萃取辅助提取中国西南地区传统食品-烟熏腊猪肉的香气成分,用气相色谱法以邻二氯苯为内标对提取的烟熏腊猪肉香气成分进行定量分析,用气相色谱-质谱联用法对提取的烟熏腊猪肉香气成分进行定性分析。共鉴定出29个化合物,烟熏腊猪肉的重要香味成分有:2,5-二苯基-3-(2-呋喃甲酰基)吡咯、二苯胺、苯并噻唑、乙酰苯酚酯、对甲苯酚、3-乙基苯酚、4-乙基愈创木酚、对-甲基-2,6-二叔丁基苯酚、硬脂醛、α-异佛尔酮、2-甲基-1-十六醇、2,6-二叔丁基-4-羟基-4-甲基-2,5-环己二烯-1-酮等。     

烟熏液(SF_2)中酚类组分的分析

酚类成分对烟熏食品的风味与防腐起最主要的作用。本文对我国首次试制出的山楂核烟熏液(SH2)经溶剂提取,分离收集其酚类组分,然后运用GC/MS(气相色谱质谱联用法)分离鉴定出21种酚类化合物,并求出了它们之间的相对含量。为综合开发利用我国特产山楂资源,改进其食用烟熏香味料的品质,提供了必要的化学依据。     

感官评价和GC-MS结合偏最小二乘回归法分析酚类化合物对腊肉烟熏风味的贡献

通过探究酚类化合物对腊肉烟熏风味的影响,确定关键烟熏风味物质。以6个烟熏腊肉和2个风干腊肉为研究对象,分别采用定量描述分析法描述气味特征和固相微萃取-气相色谱-质谱联用技术分析挥发性成分。结果表明,烟熏腊肉具有烟味、木味、灰烬味、刺鼻等4种烟熏风味,但风干腊肉不具有烟熏风味。6个烟熏腊肉样品中共鉴定出苯酚等6种烷基酚类和愈创木酚等6种愈创木基型酚类,每个样品中分别含有3～10种。2种风干腊肉中均未鉴定出酚类化合物。偏最小二乘回归(partial least-squares regression,PLSR)分析发现,除了4-甲氧基苯酚,苯酚、愈创木酚等酚类化合物对烟熏风味有较大的贡献。该研究确定了酚类化合物是腊肉中的关键烟熏风味物质,为改良食品的烟熏风味和开发烟熏液提供了理论依据。     

不同淀粉质原料对高盐稀态酱油香气品质的影响

为了研究不同淀粉质原料(面粉、麸皮)对高盐稀态酱油香气品质的影响,本文利用定量描述分析(QDA)对面粉类酱油(FSS)、麸皮类酱油(WSS)的感官特征进行分析,通过顶空-固相微萃取(HS-SPME)和液液萃取(LLE)结合气相色谱-质谱联用(GC-MS)定量对比分析了两种酱油挥发性化合物组成。FSS中酸香、土豆香、麦芽香显著性高于WSS,焦糖香、烟熏香显著性低于WSS(p0.05)。GC-MS共分离鉴定出94种挥发性化合物,其中以酸类、酮类、醛类占主要比例,HS-SPME法能萃取出较多的醛类、含硫化合物,LLE法对呋喃(酮)类、酸类化合物萃取效果较好。通过对酱油中17种关键香气活性物质定量分析以及香气活性值(OAV)的计算,有9种化合物OAV值大于20。其中3-甲基丁醛OAV值最高,HDMF、愈创木酚均有较高的OAV值,且在WSS中高于FSS,与感官分析中的焦糖香、烟熏香结果一致;FSS中2-甲基丁醛、3-甲硫基丙醛的OAV值高于WSS,与麦芽香、土豆香感官分析结果相符。     

水蒸气蒸馏法及石油醚浸提法提取灰肉红菇挥发油的化学成分分析

采用水蒸气蒸馏法及石油醚浸提法提取灰肉红菇中的挥发油,并以气相色谱-质谱联用法(GC-MS)对挥发油中的化合物进行分析鉴定.在水蒸气蒸馏法提取物中鉴定出29个化合物,占其化学成分总含量的93.58％;石油醚提取物中鉴定出36个化合物.二者相同化合物共有6种.结果表明,提取方法对于获得灰肉红菇挥发油中的化合物影响很大.     

不同分析方法在剖析塑料食品包装成分中的应用

为了剖析塑料食品包装材料的成分,采用热裂解气相色谱质谱联用仪(Py/GC-MS)、电感耦合等离子体发射光谱仪(ICP-OES)、气相色谱质谱联用仪(GC-MS)3种仪器对3种塑料食品包装进行了测试。测试结果表明Py/GC-MS可以鉴定材料的成分;ICP-OES可以测试出样品中的元素信息,并由此推断包装中所含添加剂;GC-MS可剖析塑料食品包装中的化学添加剂成分。因此,3种分析方法协同作用可以从微观角度监控塑料食品包装材料的安全性。     

龙眼木烟熏液的精制及其挥发性风味物质成分分析

为探究传统龙眼木熏制肉制品的食品安全性以及促进产业转型升级提供技术依据,以岭南特色果木-龙眼木为材料,采用干馏法制备龙眼木烟熏液并经低温净化处理,得到烟熏味浓郁的褐红色精制龙眼木烟熏液。采用气相色谱-质谱联用仪(GC-MS)分析测定了精制龙眼木烟熏液的挥发性风味成分,共鉴定出24种化合物,占烟熏液化合物的相对含量为95.66%,其中相对含量较高的有愈创木酚(31.79%)、4-甲氧基-3-甲基苯酚(11.29%)、4-乙基-2-甲氧基苯酚(8.01%)等酚类化合物以及糠醛(7.06%)等其他化合物,酚类化合物相对含量占比达到73.41%。精制烟熏液及挥发性成分中未检出苯并芘类化合物。     

烟熏腊猪肉香气成分的研究

用水蒸汽蒸馏法提取收集烟熏腊猪肉的香味成分，在蒸馏过程中，接受瓶加入200ml无水乙醚并用冰浴冷却。用无水乙醚萃取馏出物，用无水硫酸钠干燥，用高纯氮吹去溶剂浓缩至10ml。所得到的成分用气相色谱/质谱(GC／MS)法分离并分析鉴定其成分及相对含量，共鉴定出43个化合物，所鉴定的组分占挥发性成分总峰面积的98．89％，烟熏腊猪肉的关键香味成分是：愈创木酚、苯酚、5-甲基-2-甲氧基苯酚、2-甲基苯酚、4-乙基愈创木酚、2，4-二甲基苯酚、丁子香酚等。     

Experimental design-based isotope-dilution SPME-GC/MS method development for the analysis of smoke flavouring products

ABSTRACT

For the implementation of Regulation (EC) No 2065/2003 related to smoke flavourings used or intended for use in or on foods a method based on solid-phase micro extraction (SPME) GC/MS was developed for the characterisation of liquid smoke products. A statistically based experimental design (DoE) was used for method optimisation. The best general conditions to quantitatively analyse the liquid smoke compounds were obtained with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre, 60°C extraction temperature, 30 min extraction time, 250°C desorption temperature, 180 s desorption time, 15 s agitation time, and 250 rpm agitation speed. Under the optimised conditions, 119 wood pyrolysis products including furan/pyran derivatives, phenols, guaiacol, syringol, benzenediol, and their derivatives, cyclic ketones, and several other heterocyclic compounds were identified. The proposed method was repeatable (RSD% <5) and the calibration functions were linear for all compounds under study. Nine isotopically labelled internal standards were used for improving quantification of analytes by compensating matrix effects that might affect headspace equilibrium and extractability of compounds. The optimised isotope dilution SPME-GC/MS based analytical method proved to be fit for purpose, allowing the rapid identification and quantification of volatile compounds in liquid smoke flavourings.     

Some changes in an aqueous liquid smoke flavouring during storage in polythene receptacles

Aqueous liquid smoke produces a brown layer on the wall of the polythene receptacle in which it has been contained. The constituents of this brown layer have been extracted using dichloromethane and were studied by means of gas chromatography/mass spectrometry (GC/MS) and Fourier transform infrared spectroscopy (FTIR). Some changes in the liquid smoke were deduced through comparisons of data from the brown layer with the previously obtained liquid smoke data. Due to interactions between polythene molecules and compounds of the liquid smoke, some of these latter compounds migrate into the wall of the receptacle and are retained there. The extent of these migrations depends on the size of the hydrocarbon part of each compound. However, far from being harmful, this migration is useful, since compounds irrelevant from the point of view of flavour, and harmful to health are the main compounds affected by the retention on the polythene wall. Some of the adsorbed compounds have not previously been reported to be present in liquid smoke.     

芳酸果浸膏挥发性成分的分析及在卷烟中的应用

采用同时蒸馏萃取和GC/MS法定性定量分析了芳酸果浸膏挥发性成分,共鉴定出62种挥发性香味成分。同时进行了卷烟加香试验。结果表明,该香料能有效去除卷烟的杂气,改善和修饰香气,使烟气柔和细腻。     

三种Amadori化合物的热解研究

采用离线裂解装置在不同温度点对三种Amadori化合物1-L-丙氨酸-1-脱氧-D-果糖(ADF)、1-L-缬氨酸-1-脱氧-D-果糖(VDF)、1-L-脯氨酸-1-脱氧-D-果糖(PDF)分别进行裂解试验,并采用GC/MS联用技术对其产物进行初步定性研究。结果表明三种Amadori化合物在不同温度下裂解产物不同,高温时裂解产物较多;热解产物主要为醛类、吡嗪类、呋喃、呋喃酮、吡唑、吡咯、吡喃酮等杂环化合物,部分产物结构可以直接反映出Amadori化合物中糖或氨基酸的结构,这些物质是食品及卷烟烟气中重要的致香成分。      

不同类型烟熏香精对西式培根风味的影响

为研究不同类型烟熏香精对西式培根风味的影响,本研究通过感官评价和电子鼻技术对添加不同类型烟熏香精制作的西式培根进行整体风味的分析,利用固相微萃取气相色谱-质谱联用技术研究不同类型烟熏香精对西式培根挥发性风味物质的影响。结果表明,不同类型烟熏香精制作的西式培根与传统西式培根在整体风味和主体风味化合物上进行比较,乐香水溶性烟熏香精（样品5）差异最小,其次为名花烟熏膏香精（样品1）和奇华顿油溶性烟熏香精（样品3）,再次为红箭油溶性烟熏香精（样品2）,而红箭水溶性烟熏香精（样品4）差异最大。乐香水溶性烟熏香精制作的西式培根与传统西式培根（对照样）的挥发性风味物质比较接近,有愈创木酚、4-甲基愈创木酚、苯酚和2,6-二甲基苯酚等35种共有成分。其中酚类物质的种类和传统西式培根相同,而含量是传统的1.22倍,从宏观和微观上都可以达到传统西式培根的风味。     

Guaiacol and 4‐methylguaiacol accumulate in wines made from smoke‐affected fruit because of hydrolysis of their conjugates

Background and Aims: Taint in smoke‐exposed grapes have been associated with elevated levels of guaiacol and 4‐methylguaiacol. Previous research has reported guaiacol and 4‐methylguaiacol in both fruits and wines. In some cases, these compounds were not detected, or were detected at low levels in the fruit while high levels were subsequently identified during or after winemaking. Later research indicated that this was due to the presence of glycosidic conjugates. Here we report a method for the routine analysis of guaiacol and 4‐methylguaiacol released after acid hydrolysis of glycoside precursors. Methods and Results: Chardonnay, Merlot, Shiraz, Sangiovese and Cabernet Sauvignon fruits were collected following bushfire events in 2006–2007 in the King Valley wine region of NE Victoria, Australia. Gas chromatography‐mass spectrometry (GC‐MS) was used to detect free guaiacol and 4‐methylguaiacol in both fruits and wines. Low levels of free and bound forms were present in fruit not exposed to smoke. Substantial levels of free guaiacol and 4‐methylguaiacol were detected in the wines made from the smoke‐affected fruits. These compounds increased during bottle storage. Acid hydrolysis of wines and berries resulted in a several‐fold increase in free guaiacol and 4‐methylguaiacol. Conclusions: The validated GC‐MS method is suitable for monitoring free and glycosidically bound guaiacol and 4‐methylguaiacol after acid hydrolysis in both fruits and wines. Acid hydrolysis of wines provided evidence that bound volatiles, most probably glycosidically, act as reserve for guaiacol and 4‐methylguaiacol, which are released during ageing of wines. Significance of the Study: This is the first study published in a refereed journal to demonstrate that smoke taint‐associated volatiles increase during ageing of wine and bound forms of guaiacol and 4‐methylguaiacol represent an aroma reserve for smoke taint in ageing/bottled wines.     

初烤烟叶辣感关键成分的感官导向分析

为探索烟叶中的辣感关键成分,利用凝胶渗透色谱(GPC)对一种浓香型初烤烟叶的提取物进行了感官导向分离,根据滋味特征评价结果合并辣感流份,得到了辣感特征组分;采用气相色谱质谱联用技术(GC/MS)对所定位辣感特征组分进行定性分析,鉴定出4种化合物,依据定性结果用4个标样物质进行了感官评价;对辣感特征组分中烟碱进行了定量分析,依据定量分析结果复配烟碱溶液,并分别对辣感特征组分溶液和复配溶液进行了滋味分析实验(TDA);通过空白卷烟加香考察了烟碱在卷烟中的感官作用效果。结果表明:(1)4种物质中只有烟碱表现出辣感特征;(2)辣感特征组分溶液和烟碱复配溶液具有类似的辣感强度并表现出一致的稀释倍数,说明烟碱是特征组分中辣感的主要来源,是烟叶中辣感关键成分;(3)烟碱与卷烟刺激性有紧密的关联,其在显著提升烟气劲头的同时,也使口腔、喉部和鼻腔的刺激明显增强。     

沙棘化学成分提取及在卷烟中的应用

为开发新型天然烟用香料,将沙棘果实依次采用索氏提取法、加热回流法和水提醇沉法进行处理,分别得到石油醚提取物、粗黄酮以及粗多糖等成分,对石油醚提取物进行了GC/MS分析,并将提取物进行了卷烟加香试验。结果表明:①沙棘石油醚取物中共分离鉴定出49种成分,主要是酯类、羧酸类、酮类、烷烃类、醛类和醇类化合物;②提取物具有降低卷烟烟气干燥感和刺激性,改善烟气口感舒适度的作用;③与对照相比,卷烟主流烟气中的烟草特有N-亚硝胺(TSNAs)总量降低了20%左右,气相自由基和粒相自由基分别降低了约31%和26%。     

GC-MS法测定侧流卷烟烟气中挥发性化合物

采用鱼尾罩和装有剑桥滤片的捕集装置将侧流烟气中的5种挥发性化合物（1,3-丁二烯、异戊二烯、丙烯腈、苯、甲苯）捕集于甲醇溶液中, 采用四极杆GC-MS结合质谱选择性离子扫描模式（SIR）定量测定侧流卷烟烟气中5种挥发性化合物释放量。试验证明,此方法有较好的重复性:对5种挥发性化合物释放量组内测定的RSD≤3.45%,组间测定RSD≤6.27%;具有较高的灵敏度:5种挥发性化合物的检测限均低于0.13 μg /支;较高的准确性:5种挥发性化合物的回收率在93.37%～98.2%之间。      

基于静态顶空-GC/MS的加热卷烟用滤嘴载香颗粒评价研究

[目的]建立一种基于静态顶空-GC/MS的加热卷烟用滤嘴载香颗粒评价方法.[方法]采用静态顶空-GC/MS考察不同温度下4种载香颗粒中12种香味成分的释放行为,通过CH2Cl2萃取和GC/MS分析添加4种载香颗粒的加热卷烟主流烟气中香味成分释放量验证静态顶空-GC/MS评价结果.[结果]载香颗粒在加热卷烟实际抽吸降温段...